Sodium Iodide → 1-[(4-Chlorophenyl)(phenyl)methyl]-1,4-diazepane

HRID 1032966

反応式

HRID 1032966 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([CH:6](Cl)[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[I-].[Na+].[NH:18]1[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1>C(O)(C)C>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([CH:6]([N:18]2[CH2:24][CH2:23][CH2:22][NH:21][CH2:20][CH2:19]2)[C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 5238Sodium IodideHCID 68163Hexahydro-1,4-diazepineHCID 2415844-Chlorobenzhydryl chloride

生成物 1

HCID 27627031-[(4-Chlorophenyl)(phenyl)methyl]-1,4-diazepane

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

A mixture of 4-chlorobenzhydryl chloride (5.32 g, 22.4 mmol), isopropanol (80 ml) and sodium iodide (3.41 g, 22.8 mmol) was stirred at room temperature for 30 minutes. Thereto was added homopiperazine (11.2 g, 112 mmol), and the mixture was stirred at 95° C. for 18 hours. The solvent was distilled off, and the concentrate was poured into a saturated aqueous solution of sodium hydrogencarbonate and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous magnesium sulfate and evaporated. The thus-obtained crude product was used for the next reaction without purification.

後処理

  1. stirringthe mixture was stirred at 95° C. for 18 hours
  2. distillationThe solvent was distilled off
  3. additionthe concentrate was poured into a saturated aqueous solution of sodium hydrogencarbonate
  4. extractionextracted with ethyl acetate
  5. washThe extract was washed with saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customevaporated
  8. customThe thus-obtained crude product
  9. customwas used for the next reaction without purification

出典と根拠

ORDレコード
ord-677349ed45c5437db8e0af3f48f1ebbf
出典データセット
uspto-grants-1994_05
特許番号
US05308840

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